Fluidized solids contacting apparatus



Sept. 30, 1952 E. v. MURPHREE FLUIDIZED SOLIDS CONTACTING APPARATUS 5 Sheeds-Sheet 1 Filed Feb. 5, 1948 OILFEED Elgar V. murpizree Saverltor \NLET 53 MC! Qbbcrrzes Sgpt. 30, 1952 E. v. MURPHREE 2,612,438

FLUIDIZED SOLIDS. CONTACTING APPARATUS Filed Feb. 5, 1948 3 Sheets-Sheet 2 II'IIII'I'" Es'er V. mur'pbrcc Bavenbor 2: Clbborrzeg Sept. 30, 1952 E. v. MURPHREE 2,612,438

FLUIDIZED SOLIDS CONTACTING APPARATUS Filed Feb. 5, 1948 I 3 Sheets-Sheet 3 Eger' V; murpl' zr'ee. Jrzvgnbor Patented Sept. 30, 19 52 FLUIDIZED SOLIDS CONTACTING APPARATUS i Eger V. Murphree, Summit, N. .L, assignor to Standard Oil Development Company, acorporation of Delaware Application February 5, 1948, Serial No. 6,447

This invention pertains to an improved apparatus for carrying out catalytic reactions wherein finely divided catalystparticles are held in suspension in the reactant materials, and-particularly to the Stripping of adsorbed, and en trained fluidal materials from the solid catalyst particles utilized in the catalytic conversion of hydrocarbons V 7 1 There ,has been developed in recent yearsin certain catalytic operations, a method which is commonly referred to as the fluid catalyst method or technique in which finely divided solid catalyst particles are carried through a reaction zone in 'a stream of vapors undergoingreaction. 'Ifhis; method or technique is applicable to a widevariety ofcatalytic reactions and while for puroses of illustration this invention will be specifically-described in' connection with the catalytic crackingof hydrocarbons, it is to be thereto, but may be used in other catalytic processes or in other catalytic conversions of hydrocarbons, where it is desired to remove Vapors or gases from dense, fluidized, liquid-simulating mixtures of solid catalystparticles and gaseous fluids. v I

In one embodimentof the fluid catalyst technique the var-porous reactants and catalysts are introduced into the bottom of the reaction vessel, passed upwardly therethroughand are discharged into separation equipment in which the catalyst is separated from the vaporous' productsand returned to. the'reactionvessel preferably after regeneration. In, a modified or' improved design of cei'talyti'd cracking unit, the divided catalysts or contactparticles are maintained ."hindiered settling. in a dense, dry, ifluidize'd, liquid-simulat- 3 Claims. (01. 23-288) understood that the invention is not. limited .2

zone and the carbon or other combustible materials contacted with air or other regenerating gas which burns oil the carbonaceous deposits.

The contaminated, spent catalyst or contact particles withdrawn from the lower portion of the reaction zone contain adsorbed and entrained hydrocarbon vapors or gases and before regencrating the particles it is preferred practice to remove the strippable hydrocarbons in a stripping or purging operation. Theefiicieritstrippingof hydrocarbon vapors from the spent catalystin the fluid catalytic cracking operation remains.. an important and'pressing problem even after several years of commercial operation of these plants. Most of the commercial units are limited in their throughput by, the capacity of their carbonburning systems, yet 10 to 30% of the oxygen supplied to the regenerative system goes to the combustion of. gases or strippable hydrocarbons carried to the regenerator by the spent catalyst. Besides greatly reducing the feed throughput, these strippable hydrocarbons, amounting anywhere from 0.5 to 1.5 weight per cent Ion-feed, represent a sizable lossof potential products. The present invention relates to an improved design for a stripping or purging section Or zoneior a fluidized solidsreactor.

In accordance With the present invention the mixture of catalyst, or contact particles and the hydrocarbonsor other reactants are introduced into the bottom portion of a reaction zone through a hollow conical member provided with a perforated distribution plate member. Surrounding the conical member is an annular space formed by a cylindrical sleeve spaced from the inner wall of the reaction vessel. .This sleeve extends a distance above and below the distribution ing condition in the lowe-rgportion of the reaction I zone wherein hydrocarbons in vapor or gas form are contacted with the 'solidparticles. 'Thehy drocarbon'vapo'rs or gases pass upwardly through the densanuidized m'ixt'ur'e in the reactionlz one and the vaporous"products are taken overhead frcm the reactionz'one. I Duringfthe catalytic'crackihg of hydrocarbons and alsoin other catalyticfconversions ofhydro carbon materials, coke or carbona-ceousfmate'rial is deposited-bathe catalyst pr contact particles thereby reducing or I destroying their catalytic activity. The contaminatedfcr spentcatalyst must be regenerated before being rensed in the c a kin ri o her w lytic, o e at n-r mth regeneration the contaminated or spenticatalyst particl s iare .jwithdrawn .jas, a dense, fluidized mixture from the lower portion- OfrllhB. reaction plate member to form an annular stripping section atthe' bottom portion of the reaction vessel. This annular stripping section is, subdivided into a plurality'of elongated. sections by radial baffies of substantially the same length as the above-mentionedsleeve. "These bailies' form" a plurality of separate; vertically arranged, narnular stripping section into a plurality of long, narrow sections or.-cells shouldgive improved 7 stripping. .lt was found, however, that the efflcacy -of su'c,h. cellular strippers. was not nearly as good as, hadbeen expected. It is believed that upflow of catalyst occurs in a number of the cells.

It has now been found that distribution and flow of catalyst through the cells can be made more uniform, upflow of catalyst in the stripping zones can be avoided and the efiiciency of cellular strippers can be substantially improved if' an orifice is provided at thebottorn of each of the long, narrow stripping zones. for a pressure drop of about 0.1 to about lbs. per square inch across this orifice, positive flow of the catalyst particles downwardly in each of the stripping zones can be assured and flow of catalyst through each of the cells during reactor surges and gas flow variations canbe made substantiall uniform.

Reference isjmade to the accompanying drawing illustrating the present invention;

Fig. 1 represents a vertical cross-section of the lower portion of a reaction vessel embodying the present invention;

Fig. 2 'is a transverse cross-section taken substantially on the line 2"2 o f Fig. 1;

Fig. 3 is an enlarged cross-section of a single cell of thestripping section showing a suitable baflie and stripping agent inlet arrangement Figfllis a sectional view of the bottom portion of a stripper cell'showing means for distributing the stripping steam Fig; 5fi'sa' sectional view of a catalyst flow restriction orifice provided with stripping steam distributor means in closeproximity thereto: and

Fig. 6 is a plan view of the orifice andsteam di t ibut o Referring now to Figure 1 of the drawing, the reaction vessel Ill comprises an upper hemispherical dome section H a large cylindrical section [2 and a frustro conical bottom section [3 and is provided with an'inlet line: H for introducing a mixture of reactants and catalyst or contact particles. The catalyst particles are introduced into line l4 from a standpipe. or the like which is equipped with a valve l5 for controlling the rate at which the catalyst particles are supplied to line I4; from the. standpipe l5.

,The uspen i no solidca a ystor conta ing:- ticles in'reactant vapors is passed through feed 1 li'nefl4 into an inlet chamber l 'l,'comprising'an upwardlyflared wallfmember l8 and a grid memher or perforated. distribution plate 'l,9. .atjits By providing upper end. In the form of the apparatusjshown in' the drawing, the reaction vesseljiscircular in cross section and thei'grid member l9, iscircular and centrally.- arranged in. the reaction vessel. Thediameter' of the gridme'mbe'r IQ -is lessthan the internalf diameter of the reactionvessel. to

provide an annular passageway for the Withdrawal of catalyst particles from the lower portion of the reactionve'ssel. as willjbe hereinafter described in greater detail.

The velocity'oi the gaseous reactant fluid passing upwardly in the reaction vessel It ispreferably so controlled as to maintain thejsolid con- 1 tact or catalyst. particles as a dense fluidized liquid-simulatingdry mixture or bed 20 having a level indicated at 21. The vaporous reaction productsleavingthe dense bed 20 entrain-a small amount or solid catalyst particles forming a dilute phase or suspension designated at 22 in the upper portion of the reaction vessel ID.

The reaction products and entrained catalyst particles are passed through separating means 23 arranged in the upper portion of the reaction vessel. This separating means, which may be a cyclone separator or the like, separates, most of the entrained solid catalyst particles from the vaporous reaction products. The solid catalyst particles separated in the cyclone 23 are returned to the dense bed 20 through the dip leg or pipe 24 which extends below the upper level 2| of the dense bed 20. A valve for controlling returnof catalyst particles to the dense bed and means for introducing steam or other fiuidizing gas may be provided in the dip leg 2 The vaporous reaction products leaving the separat-r porous reaction products are passed to a fractionating system of separate gasoline or motor fuel .from gases and higher boiling hydrocarbon constituents.

Removal of catalyst particles from the dense phase of bed 20 is efiected through the, stripping zone generally indicated at 26 which is formed between the inner wall of the cylindrical shell I2 and a smaller diameter concentric vertically arranged sleeve 21 which surrounds the distribution plate l9 and extends some distance above and also below the said distribution plate. The upper end of the conical: wall member I8 is secured as by welding to the distribution plate 19 as well as the sleeve member 21. Secured to the bottom of sleeve member 2 is a conical "baflie or wall member 28 for reducing the eiIective volume below the inlet chamber H. The conical member 28 isarranged substantially equidistant from the'lower conical section l3 of the reactor and is provided with a vent hole 29. A- steam bleeding line 3|] is provided for supplying steam or the like, to the chamber 3| formed between walls [8; 21, and 28 in order to prevent the accumulation of; catalyst particles in said chamber.

The annular space 26 formed between the inner wall of cylindrical shell [2 and the cylindrical sleeve 2"! is subdivided into a plurality'of long andnarrow stripping zones or'sections by means of radial bafiies 32 which are substantially the same height as the cylindrical sleeve 21 and which extend from the outer wall of cylindrical sleeve 21 to the inner wall of cylindrical shell Hi The number ofjbaffies 3'2 and accordingly the number of stripping zonesprovidedmay be varled as dejsi'red. Commercial; units having an internal diameter of 2 5 30 feet may, for examplahave the annular stripping section divided intoabout 40 to '70: or even more stripping zones; or cells. An inlet 331 01 thesupply of steam or other stripping agent'is arranged at the bottom of each off the stripping cells, the, several/inlets being inf turn connectedto a manifold 34 which is cQn i'ectedby line 35 to a source of; supply of stripping gas. Thes ripp ne, ce l a n i r' b p ovided'with uit le: nc in d b l es.v n rde in rease the mixing or contactoj; the upfiow of' stripping or purging gas and the 'downflowing spent or contaminated catalyst particles; As shown the inclined baffles extendalternately from the-outer and-inner cylindrical wall member IZ-and- Z-I -in order to force the catalyst particles to follow-a sin'uouscourse downthrough the strippercells.

The bafiles could also be in therorm of alternate discs and donutbaffles.

9 In accordance with the present invention fan orifice plate 31 is provided'at the'bottom of each of the stripper cells. plates 31' are so .de-

signed asto give apressure drop or? from vv0.1 to 5.0 lbs. per square inchacrosslthe orificei l3y providing this pressure drop the flow of catalyst through the several cells is'rendered'more uni ,form and the amount of. catalyst and vaporjre cycled from the bottom of-one cell up thrbiigh lanedjacent cell is reducedifnot compvtely eliminated. Flow; of catalyst through cells'wliich are not provided witha flow restricting orifice in .bed catalyst levelvaries and.parti'cularly.d

steam through one or. mor e of: the. cells-""1 The I catalystv particle discharged fromj the s r p e ihm sh eb fi p a e 1 new downwardly 1: in the annular conical passageway 38 and are discharged intol'standpipeta which leads to a regeneratoror the like for revivifying I the spent stripped catalysts in known manner.-

lEi ures 2 and 3 show in somewhatmore detail the arrangement of stripping cell. As thereshown the radial baffles 32 are secured to theinner wall of, the cylindricalouter shell I2 and .to the outer wallcf the inner cylindrical sleeve 21 as-bywelding at. V The inclined baiiies .36 arranged in each of the stripper cells. are gsecured to, the radial battles-32 or to the cylindrical sleeve 21; or the outer cylindrical wall l2. Other bafilearran e I -,ments. -such as; alternate disc and donut baffles could be providedin order to increase; the contact of the catalyst particles and stripping agent. The orifice plates ,3! are preferably secured to the bottoms of the radial baflies 32. The orifice plates can be located at places other than the bottom of the stripper cells but placing them at higher points reduces the effective length of the stripper cell. As indicated above, theorifice plate should be designed to give a pressure drop of from 0.1

to 5.0- lbs. per square inch. ,This pressure .drop' "suflices.-,t,o even out the flowthrough the several cells and to prevent upflow o1 ,,recycling of stripped z'catalysts from the bottom; of i one strippingcell upwardly through an adjoining cell.

The steam inlet 33 to the bottom of the stripper is shown in Fig. 1 as a single nozzle. By providing for the discharge of the stripping gas or steam at a plurality of points or in several directions it is possible to improve materially the contact of catalyst particles and stripping gas. The stripping gas inlet means can take many forms. For example, it can comprise an elongated pipe having a plurality of holes drilled therein or it can be provided with one ormore side arms of the same or different size with one or more outlet holes therein or it could comprise a ring-shaped member with a plurality of openings for the discharge of stripping gas. Uniform distribution of the stripping agent can also be achieved as shown in Fig. 4 by arranging a suitable baflie such as a disc 43, provided with a plurality of openings 44 over the outlet of a single nozzle in order to break up or disperse the stream of stripping gas. A preferred arrangement is shown in Figures 5 and 6. In this embodiment, the stripping gas distributor is in the form of a ring 42 arranged directly above the catalyst restricting orifice plate 1 By making the distributor member in this 31. form, even distribution of the stripping gas is achieved and by arranging the distributor direject adj-asst the orifice, the catalyst particles aremaintained in a, fluidized condition right up to the catalyst outlet port.

The operation f 'the"app aratusi in accordance with the present invention: will now be described inv connection'iwith 'the catalytic cracking of hydrocarbons. In such catalytic cracking operations the reactant'fluidor feed stock comprise hydrocarbons such as, gas oil," reduced crude, petroleum oil, whole crudeand heavy naphtha in liquid or vapor form or partly in liquid and partly in vapor form. The catalyst or contact'particles may comprise acid treated bentonitic clay, synthetic silica-alumina or silica-magnesia gels or mixtures thereof withactivators and promoters such oxides as zinc, calcium, thorium, boron, zirconium, vanadium I chromium, molybdenum and the like or any other suitable cracking catalyst. The catalyst particles may be of any desired form, micro spherical particles being particularly convenient, The major proportion of the catalystparticlesare' ordinarily'from about 20 to micronsindiametenjj I Hot powdered catalyst uch asa silica-magnesia. cracking catalyst suppliedfrorn standpipe I5 and relatively heavy hydrocarbon oil such as.

gas oil supplied throughthe'feed inlet in 'va-poriaed or partially vaporized condition 'are pa'ssed through inlet line" ['4 into inlet chamber I 1 at temperatures between 800 and 1100 F. preferably at about 975 l. The catalyst to oil ratid'r'nay vary between about 5:1and about 30:1 by weight.

The mixtures of powdered catalyst and hydrocarbon'vapors are passed fromthe inlet chamber "11 through the distribution plate or grid l9 into the reactor proper'to form'a fluidized dry liquid simulating l' nixt'ureor dense bed 20in the reaction vessel. Velocity of the vaporized hydrocarbon materials through the bed is from about 0.6

to2. 0 ft.'per second and the density of the catalyst inthe dense'bed 20"vari'es;from about 10 to 30 lbs.

per-curt.

' Theyaporous reaction products leaving the dense bed '20 carry along small'amounts of the catalyst flnesforming a dilute phase 22, 1 The reaction-products are discharged through'the cyclone separators 23 for separating'catalyst fines -whichare returnedto the'dense bed 28 through dip-leg 24 while vapor'ous'reaction products pass overhead through line 25 to suitable recovery or treating equipment;

During the cracking operation the catalyst particles become spent by the deposition of coke or sure drop is taken and uniform distribution and flow of catalyst through the several cells is achieved and the danger of upflow occurring to carry stripped catalyst particles back into the dense bed is obviated.v The stripped catalyst par ticles pass into the conical passageway 38 and then into standpipe 39 whence they are discharged into a regenerator wherein the coke or carbonaceous deposits are burned oli rendering the catalyst particles suitable for recycling to standpipes I5 and thence into the reaction vessel l0. Steam out departing from the spiri'tof this' invention.

or other aerating gas maybe introducedinto naso- ,sageway 38 through' line n o errm beenspec'ifically described in connection with the catalytic cracking of hydrocarbons fit is to heuriderstood thatv the, apparatus .may' be used. for removing volatile material iromother 'solidcom. tact particles in other reactions such as the dehydrogenation fbutane .or butylene fractions,

aro r'it a'tizat ion 10f naphtha fractions; coking of vheavy residues andthe' like; and also may be used generally'in other reactions involving 'contact of solid particles with gaseous ior' vaporous reactants. Forlexaniple; the app'aratus eould'also be appliedin the treatirientof known hydrocarbon'materials such as the" oxidation of alcohol toia'ldehydes or acids or to the preparation of anhydrous hydrogen chloride,

. While the best known form of apnaraw has been described above, it is, to be understood that that ;is by way of illustrationonly and that various Changes and modifications maybe madewith- '-What is claimed is:

1. apparatus of the character (described including a vessel. an inlet chamber in'the bottom portion thereof for the supply of g asiform' fluid and; finely divided solids to said vessel, an out- ,l'etiforgasiform fluid in the upper part of said vessel an outlet for. "solids ,in the bottom .p'ortion, of said vesselra horizontally arranged perforated-meinber at the'upp er portion of said-inlet chamber, said. perforated member being eon- .centric with .said vessel and of smaller diam eter, a vertically disposed sleeveextending above said perforatedmember and secured-to the periphery thereof, said sleeve-being spaced from the-inner wall of said vessel to provide an annularsnace for; the withdrawal of solids, radial 'baflles arranged between the outer-wall of-said' sleeve and the inner Wall of said vessel fondividi-ng said annular spaee into a plurality of long narrow stripping cells, means 10! intro- Educing a stripping agent into the lower por- 45 .tion and substantially uniformly over the entire cross-section of each of said cells, an orifice ;pl ate horizontally arranged in the bottom ;por-

tion of each otthe said stripping cellsjbelow said ma i i e-swin s r n a e orifice plate'being construotedt dutantial pressure drop acres 'to'ni outlet Iorsolidsy a cording to claim '1 where'- ovided with -baffle means v wenth i l f a id th brin o en 'inca dite s- I nia na tuw "t e warm des ribe e a v s a'nin t :Qht ith 1W. not saidvessel-for tlle'siihplyief t. 51 151 11 sdivide zsql d 9 i v o tlet r sas l o m-fiu i theiu p r' Pa t-P9 Sa d a n m a a r n e weav he ent r mnt i efiqi Said infirmitributing L the' 'g a'sifor'mfijuid and finely solids lie-the v ssel, a oylindri'cal jsleeye surrounding said inlet chamber; "said s'leeyebei-ng spaced tram the innerwalll of said vessel were: wide an annular space ion-the withdi'ash/fail of lsoiids' trom the vessel; radi'a1 '-baffle's-arranged-- between the' outerwallet-said cylindrical sieevand the inner 'wall'of said v'ess'el for dividing said anndlar spaee intoaplurality-of long narrow stripping cells, means for1ntrod1icin'astrinping 'g'as intothe flower porti'oriof feacli o'f said-cells, a charnber at the bottom of sai'd vessel for reeeiving th solids dischared {from the" bottorn of said cells, and outlet l'ine-fdr' the discharge of'" solids connected to said last n a'r'ned chamber and' an orifice plate hori'zont'a lly arranged in: thebotto'r'n portionpf eaoh'of said cells below said' neans for "introducing"stripping agent, said 'orifice plate beins constructedto produce a substantia'l pressiire drop across said orifice't6--'c'ontrol= the' iiowbf sqlids through 's'aid cells-into saidhottinii ham- 'ber.

1 h the cells 1 yQM RPHRnm REFERENCES mun o r I ".T qi o in re e s??? e e irs i th Number 

1. AN APPARATUS OF THE CHARACTER DESCRIBED INCLUDING A VESSEL, AN INLET CHAMBER IN THE BOTTOM PORTION THEREOF FOR THE SUPPLY OF GASIFORM FLUID AND FINELY DIVIDED SOLIDS TO SAID VESSEL, AN OUTLET FOR GASIFORM FLUID IN THE UPPER PART OF SAID VESSEL, AN OUTLET FOR SOLIDS IN THE BOTTOM PORTION OF SAID VESSEL, A HORIZONTALLY ARRANGED PERFORATED MEMBER AT THE UPPER PORTION OF SAID INLET CHAMBER, SAID AT THE UPPER PORTION OF SAID INCENTRIC WITH SAID VESSEL AND OF SMALLER DIAMETER, A VERTICALLY DISPOSED SLEEVE EXTENDING ABOVE SAID PERFORATED MEMBER AND SECURED TO THE PERIPHERY THEREOF, SAID SLEEVE BEING SPACED FROM THE INNER WALL OF SAID VESSEL TO PROVIDE AN ANNULAR SPACE FOR THE WITHDRAWAL OF SOLIDS, RADIAL BAFFLES ARRANGED BETWEEN THE OUTER WALL OF SAID SLEEVE AND THE INNER WALL OF SAID VESSEL FOR DIVIDING SAID ANNULAR SPACE INTO A PLURALITY OF LONG NARROW STRIPPING CELLS, MEANS FOR INTRODUCING A STRIPPING AGENT INTO THE LOWER PORTION AND SUBSTANTIALLY UNIFORMLY OVER THE ENTIRE CROSS-SECTION OF EACH OF SAID CELLS, AN ORIFICE PLATE HORIZONTALLY ARRANGED IN THE BOTTOM PORTION OF EACH OF THE SAID STRIPPING CELLS BELOW SAID MEANS FOR INTRODUCING THE STRIPPING AGENT SAID ORIFICE PLATE BEING CONSTRUCTED TO PRODUCE A SUBSTANTIAL PRESSURE DROP ACROSS SAID ORIFICE TO CONTROL THE FLOW OF SOLIDS THROUGH THE CELLS INTO THE BOTTOM OUTLET FOR SOLIDS. 